CN115181089A - Natural nicotine purification process - Google Patents
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- CN115181089A CN115181089A CN202210697381.8A CN202210697381A CN115181089A CN 115181089 A CN115181089 A CN 115181089A CN 202210697381 A CN202210697381 A CN 202210697381A CN 115181089 A CN115181089 A CN 115181089A
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- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 82
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 title claims abstract description 81
- 229960002715 nicotine Drugs 0.000 title claims abstract description 81
- 238000000746 purification Methods 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 144
- 238000000034 method Methods 0.000 claims abstract description 57
- 238000004821 distillation Methods 0.000 claims abstract description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 238000000605 extraction Methods 0.000 claims abstract description 50
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002351 wastewater Substances 0.000 claims abstract description 36
- 238000010992 reflux Methods 0.000 claims abstract description 33
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000007599 discharging Methods 0.000 claims abstract description 22
- 241000208125 Nicotiana Species 0.000 claims abstract description 21
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 35
- 238000011084 recovery Methods 0.000 claims description 32
- 239000002904 solvent Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 239000000498 cooling water Substances 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 238000004065 wastewater treatment Methods 0.000 claims description 7
- 239000008213 purified water Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 230000035939 shock Effects 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims 2
- 239000002699 waste material Substances 0.000 abstract description 7
- 238000004062 sedimentation Methods 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- YHBIGBYIUMCLJS-UHFFFAOYSA-N 5-fluoro-1,3-benzothiazol-2-amine Chemical compound FC1=CC=C2SC(N)=NC2=C1 YHBIGBYIUMCLJS-UHFFFAOYSA-N 0.000 description 7
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 239000003571 electronic cigarette Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000208134 Nicotiana rustica Species 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000003113 alkalizing effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005586 smoking cessation Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/04—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention designs a natural nicotine purification process, which is a production process for purifying a tobacco extract raw material with 40% of nicotine content to the nicotine content of more than or equal to 99.95% and the nicotine yield of more than or equal to 99.5% through the procedures of emulsifier resistant preparation, alkalization treatment, extraction separation, standing sedimentation, wastewater separation, distillation desolventization and rectification purification. The method specifically comprises the following steps: mixing raw materials, water and caustic soda according to a set proportion and a set program to prepare an extraction liquid, mixing the extraction liquid with normal hexane to prepare an extraction mixed liquid, standing and settling for 60 hours, discharging wastewater and recovering clear liquid in emulsion after the extraction mixed liquid is layered, and then distilling and recycling the normal hexane in the clear liquid, wherein the distilled raw materials are subjected to high-proportion reflux rectification, and the rectification scheme comprises the following steps: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction, and recovering heavy clean oil to obtain the high-purity nicotine finished product. Breaks through the limitations of low purity, low yield, large waste discharge and the like of the existing purification process, and has extremely high popularization value.
Description
Technical Field
The invention relates to a process for purifying natural nicotine, in particular to a production process for purifying 40 percent nicotine sulfate raw material to the purity of more than 99.95 percent of the natural nicotine and the yield of the nicotine in the raw material to be more than 99.5 percent through the process flow of the invention, which belongs to the technical field of the equipment of the process for purifying the effective components of natural plants.
Background
The nicotine is an effective component for cigarettes in the tobacco raw materials, and the natural nicotine product is mainly used as a functional additive of the electronic cigarette atomized liquid, and is used in small amount as a smoking cessation medicament and an insecticide in medicine. The natural nicotine is obtained by processing a small amount of tobacco residue wastes such as tobacco powder, broken stems, tobacco leaf fragments and the like generated in the tobacco processing process. The obtained natural nicotine has small amount of impurities, which are mainly flavor substances in tobacco. Due to differences in many aspects such as production areas, varieties and natural fermentation degrees of tobacco leaves, the components of the impurities are different, and due to factors of the impurities, the fragrance and the aroma of the natural nicotine raw materials used in the electronic cigarette industry are different to a certain extent, that is, the purity of the natural nicotine raw materials is insufficient, so that the fragrance of the electronic cigarette atomized liquid is influenced to a great extent (the consistency is poor), and the product quality of the electronic cigarette is further influenced.
The prior domestic and overseas well-known natural nicotine purification process comprises the following steps:
40% nicotine sulfate → alkalization treatment → extraction separation → distillation desolventizing → rectification and purification → sealed storage
In the process, 40% nicotine sulfate refers to: the liquid natural nicotine with the purity higher than 99 percent can be obtained by alkalizing, extracting, distilling and rectifying the raw material of the tobacco extract with the liquid natural nicotine content of about 40 percent. Because the raw materials belong to valuables and have toxic hazard to water ecology, and the residues after extraction can be discharged after being treated, the improvement of purity and the increase of recovery rate are always important targets continuously pursued in the industry.
The existing purification process has the following defects:
1. because a direct separation mode is adopted after extraction, enough settling separation time required for settling and separating substances in the materials is not given, so that a waste water layer contains the solvent and nicotine, and water-soluble impurities in the solvent can not be effectively separated. Under the condition of water, the boiling point of nicotine is greatly reduced, so that the recovery rate of natural nicotine is insufficient, and the final comprehensive recovery rate is only about 83.5 percent.
2. In the rectification purification process, because a forced reflux pipe is not arranged, although a small amount of rectification liquid naturally reflows in a rectification tower pipe in the rectification process, the ratio of the reflowing amount to the collection amount of a finished product is too small (< 10%), the impurities with high boiling points in the material are not easily removed, and the final purity cannot reach an ideal target. Based on this, in the international and domestic industries, the purity of natural nicotine purified by the process is only about 99.0%, and the highest purity can not be higher than 99.8%.
3. In the process production process, the recovery rate of natural nicotine is an important index, and one of the adverse factors of insufficient recovery rate is that valuable raw materials are wasted, and the purification cost is increased; secondly, the pollution discharge pressure of the unrecycled raw materials which can not be recycled is increased, and the waste treatment cost is further increased.
The related processes in the aspect of purifying natural nicotine at home and abroad are searched, and no introduction or open documents in the aspect of comprehensive recovery rate of more than or equal to 99.5 percent and/or product purity of more than or equal to 99.95 percent exist.
Disclosure of Invention
The invention aims to design a natural nicotine purification process aiming at the problems in the prior art, and the process is a production process for purifying a liquid 40% nicotine sulfate raw material, namely a tobacco extract with 40% nicotine content, to a natural nicotine tobacco raw material with the purity of more than or equal to 99.95% through the process flow of the invention, and the nicotine yield is more than or equal to 99.5%.
The technical scheme of the invention is as follows: a process for purifying natural nicotine is characterized by comprising the following steps:
the process comprises the following steps: preparing an anti-emulsifier, performing alkalization treatment, extracting and separating, standing and settling, separating wastewater, distilling and desolventizing, and rectifying and purifying; the devices or equipment required in each process comprise: the device comprises a dosing tank 1, a mixing tank 2, an extraction tank 3, a settling tank 4, a pipeline filter 5, a clear liquid receiving tank 6, a pipeline viewing mirror 7, a No. 1 delivery pump 8, a distillation tower 9, a first condenser 10, a solvent recovery tank 11, a No. 2 delivery pump 12, a solvent cache tank 13, a feeding cache tank 14, a rectification tower 15, a rectification tower pipe 16 with a built-in stainless steel wire mesh filler, a second condenser 17, a condensate buffer tank 18, an automatic forced reflux distributor 19, a qualified product receiving tank 20, a unqualified product receiving tank 21, a reflux pipe 22, a sample collection valve 24 arranged at the front part of the reflux pipe 22 and a rectification liquid collection pipe 25; the system also comprises a controller used for detecting and controlling the operation of each device or equipment: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system; the 1# delivery pump is used for conveying clear liquid, the 2# delivery pump is used for conveying recyclable n-hexane, and the vacuum pump is used for pumping gas in a specified container and/or introducing required materials under negative pressure; the condensate buffer tank 18 receives the material flowing out of the second condenser 17 and flows to the automatic forced reflux distributor 19, a one-inlet and two-outlet proportion adjusting three-way valve is arranged in the automatic forced reflux distributor 19, one outlet of the three-way valve is communicated with the upper part of the rectifying tower pipe 16 through a reflux pipe 22, and the other outlet of the three-way valve is connected to a qualified product receiving tank 20 or a unqualified product receiving tank 21 through a rectifying liquid collecting pipe 25; constant-temperature heating jackets are arranged outside the distillation tower 9 and the rectifying tower 15, and heat exchange tubes are arranged inside the first condenser 10 and the second condenser 17;
the purification process comprises the following specific steps:
stp1, preparation of an anti-emulsifier: injecting a set amount of purified water into the batching tank 1 in a negative pressure mode, and then slowly adding a set amount of caustic soda with the purity of more than or equal to 98 percent while stirring to prepare an anti-emulsifier; controlling the adding time of the caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifier in the batching tank 1 is reduced to 40-45 ℃;
stp2, alkalization treatment: liquid 40% nicotine sulfate raw material to be purified, namely: injecting the tobacco extract with nicotine content of 40% into a mixing tank 2 in a negative pressure suction mode, and slowly adding the anti-emulsifying agent prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90 to 120min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract;
stp3, extraction and separation: injecting a set amount of normal hexane into the extraction tank 3 in a negative pressure mode, and adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to prepare an extraction mixed solution;
stp4, standing and settling: conveying the extraction mixed solution prepared according to stp3 into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free settled under the state of standing in settling cask 4, and the material of final extraction mixed liquor realizes free layering because of the density difference, wherein: the low-density clear liquid is positioned at the upper layer, the medium-density emulsified liquid is positioned at the middle layer, and the high-density waste water is positioned at the lower layer; the clear liquid is n-hexane solution extracted with nicotine;
setting: the free settling time of the extraction mixed solution in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: observing the liquid level and the layering condition in the settling tank 4 after stp4 reaches the set standing and settling time, and discharging the wastewater through a valve arranged at the bottom of the settling tank 4 until the liquid level of the wastewater in the settling tank 4 is lower than the height of a clear liquid discharge hole arranged on the settling tank 4; respectively discharging clear liquid, waste water and emulsion in a gravity self-flow mode, discharging the clear liquid into a clear liquid receiving tank 6, discharging the waste water into a temporary waste water treatment container, and discharging the emulsion for additional storage;
stp6, distillation desolventizing; conveying the clear liquid stored in the clear liquid receiving tank 6 to a distillation tower 9 in batches by a No. 1 material conveying pump, separating n-hexane in the clear liquid in an evaporation and condensation mode, temporarily storing the separated n-hexane in a solvent recovery tank 11 while distilling, and conveying the n-hexane to a solvent cache tank 13 by a No. 2 material conveying pump for extracting the raw materials of the next batch;
after the distillation desolventizing process is completed, what remains in the distillation column is: crude absolute oil with nicotine purity of more than or equal to 95 percent is delivered to the feeding buffer tank 14 in a negative pressure delivery mode;
setting: the distillation temperature of the clear liquid in the distillation tower 9 is 80 to 140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank 11 is determined to be less than 1% of the maximum flow, closing an emptying valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuum-pumping pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not fall and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then feeding nitrogen into the distillation tower to break the air, and closing the heating source;
stp7, rectification and purification: the rectification and purification comprises five links, which are respectively: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction and recovering heavy clean oil;
in the operation process, the flow ratio I value between the return pipe 22 and the rectification liquid pipe 25 can be adjusted by adjusting a proportional adjustment three-way valve arranged in the automatic forced return distributor 19;
the specific operation process of the step is as follows:
a. feeding and equilibrium temperature: firstly, setting: the return pipe 22 is fully opened, the rectification liquid collecting pipe 25 is closed, and the liquid flows through the condensate buffer tank 18 and is totally returned to the upper end of the rectification tower pipe 16, namely the value I is infinite, and the vacuum degree in the rectification tower 15 is higher than-0.09 Mpa; and pumping the crude clean oil fed into the buffer tank 14 into the rectifying tower 15, heating the crude clean oil to 135 +/-1 ℃, and setting the continuous evaporation and reflux time of the crude clean oil in the rectifying tower 15 under the constant temperature state as follows: 3~4 hours;
b. collecting front fractions: a rectification liquid sample is extracted from the sample collection valve 24 at regular time and analyzed, when the content of single high-boiling point impurities in the rectification liquid is less than or equal to 100mg/kg, the I value is adjusted to be = (5~3), and the material flowing out of the rectification liquid pipe 25 is led into the unqualified product receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95 percent, the front-end distillation collection process is finished;
c. collecting high-purity nicotine fractions: keeping the value I as the set value in the step b, continuing rectification, when the purity of the nicotine in the collected sample is more than or equal to 99.95 percent, and the content of single high-boiling-point impurities is more than 100mg/kg but less than 200mg/kg, immediately guiding the material flowing out of the rectification liquid pipe 25 into the qualified product receiving tank 20, stopping collecting the high-purity nicotine fraction until the purity of the nicotine in the sample is reduced from high to 99.95 percent, and closing a feeding valve for communicating the qualified product receiving tank 20 with the rectification liquid pipe 25;
d. and (3) collecting the after fraction: after step c is finished, adjusting the value I =0, namely cutting off reflux, and guiding the material flowing out of the rectification liquid pipe 25 into the unqualified product receiving tank 21; the rectifying tower 15 continues to rectify according to the temperature set in the step a until the temperature in the rectifying tower 15 does not rise or fall reversely, and then rectification is finished; finally, the unqualified rectification liquid collected by the unqualified product receiving tank 21 flows back to the clear liquid receiving tank 6;
e. and (3) heavy clean oil recovery: after the rectification is finished, nitrogen is used for emptying and discharging heavy clean oil remained in the rectifying tower 15, and then the next rectification circulation process is carried out. Preferably, the lower parts of the shells of the mixing tank 1 and the mixing tank 2 are provided with cooling jackets for accelerating cooling of materials stored in the mixing tank 2 and the mixing tank 1, and the cooling jackets are connected with a cooling water circulation pipeline arranged outside; the first condenser 10 and the second condenser 17 are also respectively connected with a cooling water circulation pipeline arranged outside; setting: the water inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the water return temperature is less than or equal to 35 ℃;
preferably, the lower parts of the shells of the qualified product receiving tank 20 and the unqualified product receiving tank 21 are provided with freezing jackets for storing the materials in the qualified product receiving tank 20 and the unqualified product receiving tank 21 under the low temperature condition, and the freezing jackets are connected with a chilled water circulation pipeline arranged outside; setting: the water inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the water return temperature is less than or equal to 10 ℃;
further, in the stp1, set are: the weight ratio of the purified water to the caustic soda is 4: (0.8 to 1.2); in stp2, the following are set: the weight ratio of the anti-emulsifier to the tobacco extract with the nicotine content accounting for 40% is 5: (3.5 to 4.5); in stp3, the following are set: the weight ratio of the n-hexane to the extract is 13: (8 to 10);
further, fan-shaped propeller stirrers are arranged in the batching tank 1 and the mixing tank 2, and the fan-shaped propeller stirrers are set in the work: the rotating speed of the fan-shaped propeller stirrer is as follows: 90 to 120 revolutions per minute.
Preferably, three groups of stirrers which are coaxially distributed along the vertical direction are arranged in the extraction separation tank 3 and the distillation tower 9, and a fan-shaped propeller stirrer, a frame-type stirrer and a fan-shaped propeller stirrer are sequentially arranged from top to bottom, and the rotating speeds of the three groups of stirrers are set in the work: 80 to 160 revolutions per minute.
Further, in the stp5, the discharged emulsion is subjected to a shock demulsification method to further separate a clear liquid remaining in the emulsion, the separated clear liquid is introduced into a clear liquid receiving tank 6, and the wastewater discharged into the temporary wastewater treatment container is introduced into a wastewater innocent treatment device.
Furthermore, in the stp7, a pipe pump or a metering pump is connected in series between the automatic forced reflux distributor 19 and the reflux pipe 22, and a centralized control system precisely controls the reflux amount of the rectification liquid through the pipe pump or the metering pump.
The invention has the advantages and beneficial effects that:
1. compared with the prior art, the technical scheme of the invention has the most outstanding innovation points that: the standing and settling process is added, and the settling time is set to be more than 60 hours, so that the precipitation and separation of the extracted materials are facilitated, the comprehensive recovery rate of the natural nicotine in the raw materials is improved to be more than 99.5%, the raw materials are favorably used up, and the environmental protection pressure is favorably reduced.
2. By adopting the technical scheme of the invention, the reflux quantity I value set in the rectification process is 5~3 which is greatly higher than that of the prior art which only depends on a natural reflux mode, so that the purity of finished product nicotine can reach more than 99.95 percent, and the purity requirement of a final user on the product can be met.
3. The technical scheme of the invention has the advantages of less required equipment, easy realization of automatic operation, low energy consumption of unit products, high comprehensive utilization rate of raw materials, less waste discharge and low cost for waste treatment.
4. The technical scheme of the invention has high popularization value.
Drawings
FIG. 1 is a process flow diagram of the technical solution of the present invention;
FIG. 2 is a diagram of an apparatus configuration according to an embodiment of the present invention;
FIG. 3 is an enlarged schematic view of a condensing and refluxing apparatus of the purification portion of FIG. 2;
FIG. 4 is a process flow diagram according to one embodiment of the present invention.
Description of the reference symbols in the drawings:
in fig. 2 and 3, 1-proportioning tank, 2-mixing tank, 3-extraction tank, 4-settling tank, 5-pipeline filter, 6-clear liquid receiving tank, 7-pipeline sight glass, 8-1 # delivery pump, 9-distillation tower, 10-condenser one, 11-solvent recovery tank, 12-2 # delivery pump, 13-solvent buffer tank, 14-feed buffer tank, 15-distillation tower, 16-distillation tower pipe, 17-condenser two, 18-condensate buffer tank, 19-automatic forced reflux distributor, 20-qualified product receiving tank, 21-unqualified product receiving tank, 22-reflux pipe, 24-sample collection valve, 25-rectification liquid collection pipe.
Detailed Description
Embodiments of the invention will be further described with reference to the accompanying drawings, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below are exemplary and are intended to be illustrative, but not limiting, of the present invention, and any modifications, equivalents, or improvements made within the spirit and principle of the present invention, which are not described in detail in the technical solutions below, are known in the art, and are intended to be included within the scope of the claims of the present invention.
Referring to fig. 1 to 3, the invention relates to a natural nicotine purification process, which comprises the following steps: preparing an anti-emulsifier, performing alkalization treatment, extracting and separating, standing and settling, separating wastewater, distilling and desolventizing, and rectifying and purifying.
The devices or equipment required in each process comprise: the device comprises a dosing tank 1, a mixing tank 2, an extraction tank 3, a settling tank 4, a pipeline filter 5, a clear liquid receiving tank 6, a pipeline viewing mirror 7, a No. 1 delivery pump 8, a distillation tower 9, a first condenser 10, a solvent recovery tank 11, a No. 2 delivery pump 12, a solvent cache tank 13, a feeding cache tank 14, a rectification tower 15, a rectification tower pipe 16 with a built-in stainless steel wire mesh filler, a second condenser 17, a condensate buffer tank 18, an automatic forced reflux distributor 19, a qualified product receiving tank 20, a unqualified product receiving tank 21, a reflux pipe 22, a sample collection valve 24 arranged at the front part of the reflux pipe 22 and a rectification liquid collection pipe 25; the system also comprises a controller used for detecting and controlling the operation of each device or equipment: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system.
The 1# delivery pump is used for conveying clear liquid, the 2# delivery pump is used for conveying recyclable n-hexane, and the vacuum pump is used for pumping gas in a specified container and/or introducing required materials under negative pressure; the condensate buffer tank 18 receives the material flowing out of the second condenser 17 and flows to the automatic forced reflux distributor 19, a one-inlet and two-outlet proportion adjusting three-way valve is arranged in the automatic forced reflux distributor 19, one outlet of the three-way valve is communicated with the upper part of the rectifying tower pipe 16 through a reflux pipe 22, and the other outlet of the three-way valve is connected to a qualified product receiving tank 20 or a unqualified product receiving tank 21 through a rectifying liquid collecting pipe 25; constant-temperature heating jackets are arranged outside the distillation tower 9 and the rectifying tower 15, and heat exchange tubes are arranged inside the first condenser 10 and the second condenser 17.
Be provided with fan-shaped propeller agitator in batching jar 1, the compounding jar 2, the setting in the work: the rotating speed of the fan-shaped propeller stirrer is as follows: 90 to 120 revolutions per minute; three groups of stirrers which are coaxially distributed along the vertical direction are arranged in the extraction separation tank 3 and the distillation tower 9, and a fan-shaped propeller stirrer, a frame-type stirrer and a fan-shaped propeller stirrer are sequentially arranged from top to bottom, and the rotating speeds of the three groups of stirrers are set in the working process: 80 to 160 revolutions per minute.
The lower parts of the shells of the mixing tank 1 and the mixing tank 2 are provided with cooling jackets which are used for accelerating the cooling of the materials stored in the mixing tank 1 and the mixing tank 2, and the cooling jackets are connected with a cooling water circulation pipeline arranged outside; the first condenser 10 and the second condenser 17 are also respectively connected with a cooling water circulation pipeline arranged outside; setting: the water inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the water return temperature is less than or equal to 35 ℃.
The lower parts of the shells of the qualified product receiving tank 20 and the unqualified product receiving tank 21 are provided with freezing jackets, the freezing jackets are used for storing materials in the qualified product receiving tank 20 and the unqualified product receiving tank 21 under the low-temperature condition, and the freezing jackets are connected with a chilled water circulating pipeline arranged outside; setting: the water inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the water return temperature is less than or equal to 10 ℃.
The purification process comprises the following specific steps:
stp1, preparation of an anti-emulsifier: injecting a set amount of purified water into the batching tank 1 in a negative pressure mode, and then slowly adding a set amount of caustic soda with the purity of more than or equal to 98 percent while stirring to prepare an anti-emulsifier; controlling the adding time of the caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifier in the batching tank 1 is reduced to 40-45 ℃; setting: the weight ratio of the purified water to the caustic soda is 4: (0.8 to 1.2);
stp2, alkalization treatment: liquid 40% nicotine sulfate raw material to be purified is prepared, namely: injecting the tobacco extract with nicotine content of 40% into a mixing tank 2 in a negative pressure suction mode, and slowly adding the anti-emulsifying agent prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90 to 120min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract; setting: the weight ratio of the anti-emulsifier to the tobacco extract with the nicotine content accounting for 40% is 5: (3.5 to 4.5);
stp3, extraction and separation: injecting a set amount of normal hexane into the extraction tank 3 in a negative pressure mode, and adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to obtain an extraction mixed solution; setting: the weight ratio of the n-hexane to the extract is 13: (8 to 10);
stp4, standing and settling: conveying the extraction mixed solution prepared according to stp3 into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free settled under the state of standing in settling cask 4, and the material of final extraction mixed liquor realizes free layering because of the density difference, wherein: the low-density clear liquid is positioned at the upper layer, the medium-density emulsified liquid is positioned at the middle layer, and the high-density waste water is positioned at the lower layer; the clear liquid is n-hexane solution extracted with nicotine;
setting: the free settling time of the extraction mixed solution in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: observing the liquid level and the layering condition in the settling tank 4 after stp4 reaches the set standing and settling time, and discharging the wastewater through a valve arranged at the bottom of the settling tank 4 until the liquid level of the wastewater in the settling tank 4 is lower than the height of a clear liquid discharge hole arranged on the settling tank 4; respectively discharging clear liquid, waste water and emulsion in a gravity self-flow mode; discharging the clear liquid into a clear liquid receiving tank 6, discharging the wastewater into a temporary wastewater treatment container, further separating the clear liquid remaining in the emulsion by a vibration demulsification method after the emulsion is discharged, introducing the separated clear liquid into the clear liquid receiving tank 6, and introducing the wastewater discharged into the temporary wastewater treatment container into a wastewater harmless treatment device;
stp6, distillation desolventizing; conveying the clear liquid stored in the clear liquid receiving tank 6 to a distillation tower 9 in batches by a No. 1 material conveying pump, separating n-hexane in the clear liquid in an evaporation and condensation mode, temporarily storing the separated n-hexane in a solvent recovery tank 11 while distilling, and conveying the n-hexane to a solvent cache tank 13 by a No. 2 material conveying pump for extracting the raw materials of the next batch;
after the distillation desolventizing process is completed, what remains in the distillation column is: crude absolute oil with nicotine purity of more than or equal to 95 percent is delivered to the feeding buffer tank 14 in a negative pressure delivery mode;
setting: the distillation temperature of the clear liquid in the distillation tower 9 is 80 to 140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank 11 is determined to be less than 1% of the maximum flow, closing an emptying valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuum-pumping pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not fall and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then feeding nitrogen into the distillation tower to break the air, and closing the heating source;
stp7, rectification and purification: the rectification and purification comprises five links, which are respectively: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction, and recovering heavy clean oil;
in the operation process, the flow ratio I value between the return pipe 22 and the rectification liquid pipe 25 can be adjusted by adjusting a proportional adjustment three-way valve arranged in the automatic forced return distributor 19;
the specific operation process of the step is as follows:
a. feeding and equilibrium temperature: firstly, setting: the return pipe 22 is fully opened, the rectification liquid collecting pipe 25 is closed, and the liquid flows through the condensate buffer tank 18 and is totally returned to the upper end of the rectification tower pipe 16, namely the value I is infinite, and the vacuum degree in the rectification tower 15 is higher than-0.09 Mpa; and pumping the crude clean oil fed into the buffer tank 14 into the rectifying tower 15, heating the crude clean oil to 135 +/-1 ℃, and setting the continuous evaporation and reflux time of the crude clean oil in the rectifying tower 15 under the constant temperature state as follows: 3~4 hours;
b. collecting front fractions: a rectification liquid sample is extracted from the sample collection valve 24 at regular time and analyzed, when the content of single high-boiling point impurities in the rectification liquid is less than or equal to 100mg/kg, the I value is adjusted to be = (5~3), and the material flowing out of the rectification liquid pipe 25 is led into the unqualified product receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95 percent, the collection process of the front distillation is finished;
c. collecting high-purity nicotine fractions: keeping the value I as the set value in the step b, continuing rectification, when the purity of the nicotine in the collected sample is more than or equal to 99.95 percent, and the content of single high-boiling-point impurities is more than 100mg/kg but less than 200mg/kg, immediately guiding the material flowing out of the rectification liquid pipe 25 into the qualified product receiving tank 20, stopping collecting the high-purity nicotine fraction until the purity of the nicotine in the sample is reduced from high to 99.95 percent, and closing a feeding valve for communicating the qualified product receiving tank 20 with the rectification liquid pipe 25; d. and (3) collecting the after fraction: after step c is finished, adjusting the value I =0, namely cutting off reflux, and guiding the material flowing out of the rectification liquid pipe 25 into the unqualified product receiving tank 21; the rectifying tower 15 continues to rectify according to the temperature set in the step a until the temperature in the rectifying tower 15 does not rise or fall reversely, and then rectification is finished; finally, the unqualified rectification liquid collected by the unqualified product receiving tank 21 flows back to the clear liquid receiving tank 6;
e. and (3) heavy clean oil recovery: after the rectification is finished, nitrogen is used for emptying and discharging heavy clean oil remained in the rectifying tower 15, and then the next rectification circulation process is carried out.
The technical solution of the present invention is further illustrated by the following specific example
The first embodiment is as follows:
referring to the attached fig. 4, fig. 2 and fig. 3, the raw material of the tobacco extract with 40% nicotine content required to be purified at a single time is 400kg, and by adopting the purification process of the invention, the other main raw materials are respectively required: 100kg of caustic soda with the purity of more than or equal to 98 percent, 400kg of tap water, 1300kg of normal hexane, a small amount of nitrogen, and cooling water and chilled water required by the production process are recycled and almost have no loss. The chilled water is prepared by a refrigerating unit, and the setting is as follows: the inlet and return water temperatures of the chilled water are respectively as follows: selecting running water as cooling water at 5 ℃ and 10 ℃, and setting the water inlet temperature and the water return temperature of the cooling water as follows: the heating source required by the distillation and rectification processes is a heat conduction oil circulating pipeline at the temperature of 20 ℃ and 30 ℃, and the setting is as follows: the oil inlet temperature and the oil return temperature of the heat conduction oil are respectively as follows: 160 ℃ and 155 ℃. The specific purification process comprises the following steps:
stp1, preparation of an anti-emulsifier: injecting tap water into the batching tank 1 in a negative pressure mode, and then slowly adding caustic soda while stirring to prepare an anti-emulsifier; controlling the adding time of the caustic soda for 35min, stirring until the caustic soda is completely dissolved, continuing stirring until the anti-emulsifier in the batching tank 1 is dissolved, and cooling and circulating the anti-emulsifier in the batching tank 1 to be below 40 ℃ by matching with tap water outside the batching tank; a fan-shaped arc stirrer is adopted, the diameter of the fan blades is 400mm, and the stirring speed is 100 r/min.
stp2, alkalization treatment: injecting raw materials to be purified into a mixing tank 2 in a negative pressure suction mode, and slowly adding the anti-emulsifier prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be 40min, and continuously stirring for 90min after the anti-emulsifying agent is completely added into the tobacco extract; to prepare an extract.
stp3, extraction and separation: firstly, 1300kg of normal hexane is injected into the extraction tank 3 in a negative pressure mode, and then the extraction liquid prepared according to stp2 is added while stirring; controlling the adding time of the extract liquor for 60min, and continuously stirring for 90min after all the extract liquor is added; finishing the extraction process to prepare an extraction mixed solution.
stp4, standing and settling: the extraction mixed solution prepared according to the stp3 is completely conveyed into a settling tank 4 in a negative pressure mode; the extraction mixed liquor is free settled for 60h in the settling tank 4 under the standing state, and the material of the final extraction mixed liquor is free layered due to density difference, wherein: the low-density clear liquid is positioned at the upper layer, the medium-density emulsified liquid is positioned at the middle layer, and about 700kg of high-density wastewater is positioned at the lower layer; the clear liquid is n-hexane solution extracted with nicotine.
stp5, wastewater separation: after the sedimentation process is finished, observing the liquid level and the layering condition in the sedimentation tank 4 through a pipeline sight glass 7 arranged on the sedimentation tank 4, and discharging partial wastewater through a valve arranged at the bottom of the sedimentation tank 4 until the liquid level of the wastewater is lower than the height of a clear liquid discharge hole arranged on the sedimentation tank 4; respectively discharging clear liquid, waste water and emulsion in a gravity self-flow mode; and discharging the clear liquid into a clear liquid receiving tank 6, discharging the wastewater into a temporary wastewater treatment container, further separating the clear liquid remaining in the emulsion by a vibration demulsification method after the emulsion is discharged, introducing the separated clear liquid into the clear liquid receiving tank 6, and introducing the wastewater discharged into the temporary wastewater treatment container into a wastewater harmless treatment device.
Stp6, distilling and removing a solvent; the clear liquid stored in the clear liquid receiving tank 6 is conveyed to the distillation tower 9 in batches through the No. 1 delivery pump, normal hexane in the clear liquid is separated in an evaporation and condensation mode, the separated normal hexane is temporarily stored in the solvent recovery tank 11 while distillation is carried out, and then the clear liquid is conveyed to the solvent cache tank 13 through the No. 2 delivery pump to be used for extracting the nicotine sulfate raw material in the next batch. Setting: the distillation temperature of the clear liquid in the distillation tower 9 is 100 + -1 deg.C, and after the distillation desolventizing process is completed, the nicotine in the distillation tower 9 has a purity not lower than that of nicotine95% crude neat oil, which is then transferred to the feed buffer tank 14 in a negative pressure transfer.
In the later stage of distillation, when the input flow of the solvent recovery tank 11 is determined to be less than 1% of the maximum flow, closing an emptying valve arranged at the outlet of the solvent recovery tank 11, communicating the solvent recovery tank 11 with an external vacuum-pumping pipeline, and continuously distilling under the negative pressure condition until a thermometer arranged at the top of the distillation tower shows that the temperature does not fall and rise reversely, namely, the normal hexane in the clear liquid is completely distilled; then, nitrogen is fed into the distillation tower to be broken, and the heating source is closed.
Stp7, rectification and purification: the rectification and purification comprises four links, which are respectively: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction and recovering heavy clean oil.
In the operation process, the flow ratio I between the return pipe 22 and the rectification liquid pipe 25 can be adjusted by adjusting a proportional adjustment three-way valve arranged in the automatic forced return distributor 19.
The specific operation process of the step is as follows:
a. feeding and equilibrium temperature: firstly, setting: the return pipe 22 is fully opened, the rectification liquid collecting pipe 25 is closed, and the liquid flows through the condensate buffer tank 18 and is totally returned to the upper end of the rectification tower pipe 16, namely the value I is infinite, and the vacuum degree in the rectification tower 15 is higher than-0.09 Mpa; and pumping the crude clean oil fed into the buffer tank 14 into the rectifying tower 15, heating the crude clean oil to 135 +/-1 ℃, and setting the continuous evaporation and reflux time of the crude clean oil in the rectifying tower 15 under the constant temperature state as follows: 3~4 hours.
b. Collecting front fractions: regularly extracting a rectification liquid sample from the sample collecting valve 24 and analyzing, when the content of single high-boiling-point impurities in the rectification liquid is less than or equal to 100mg/kg, adjusting the I value =5, and guiding the material flowing out of the rectification liquid pipe 25 into the unqualified product receiving tank 21; when the purity of nicotine in the collected sample is more than or equal to 99.95 percent, the collection process of the front distillation is finished; this process takes approximately 3~5 hours.
c. Collecting high-purity nicotine fractions: keeping the value I as the set value in the step b, continuing rectification, when the purity of the nicotine in the collected sample is more than or equal to 99.95 percent, and the content of single high-boiling-point impurities is more than 100mg/kg but less than 200mg/kg, immediately guiding the material flowing out of the rectification liquid pipe 25 into the qualified product receiving tank 20, stopping collecting the high-purity nicotine fraction until the purity of the nicotine in the sample is reduced from high to 99.95 percent, and closing a feeding valve for communicating the qualified product receiving tank 20 with the rectification liquid pipe 25; the process takes about 13 to 15 hours. d. And (3) collecting the after fraction: after step c is finished, adjusting the value I =0, namely closing the return pipe 22, and guiding the material flowing out of the rectification liquid pipe 25 into the unqualified product receiving tank 21; the rectifying tower 15 continues to rectify according to the temperature set in the step a until the temperature in the rectifying tower 15 does not rise or fall reversely, and then rectification is finished; finally, the unqualified rectification liquid collected by the unqualified product receiving tank 21 flows back to the clear liquid receiving tank 6; this process takes approximately 30 to 50 minutes.
e. And (3) heavy clean oil recovery: after the rectification, about 5kg of heavy clean oil remaining in the rectifying tower 15 is evacuated and discharged by using nitrogen gas, and then enters the next rectification cycle.
Compared with the prior art, the technical scheme of the invention has the outstanding innovation points that the standing and settling process is added, the settling time is set to be more than 60 hours, the precipitation and separation of the extracted materials are facilitated, the comprehensive recovery rate of the natural nicotine in the raw materials is improved to be more than 99.5%, the raw materials are favorably used up, and the environmental protection pressure is favorably relieved; secondly, the reflux quantity I value set in the rectification procedure is 5 to 2.5, which is greatly higher than that of the prior art which only depends on a natural reflux mode, so that the purity of the finally obtained nicotine finished product can reach more than 99.95 percent, and the purity requirement of a final user on the product is greatly adapted; the technical scheme of the invention has the advantages of less required equipment, easy realization of automatic operation, low energy consumption of unit products, high comprehensive utilization rate of raw materials, less waste discharge, low cost for waste treatment and high popularization value.
In the present invention, unless otherwise specifically stated or limited, the terms "mounted," "connected," "fixed," "secured," and the like are to be construed broadly, e.g., as meaning a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "above," and "over" a second feature may be directly on or obliquely above the second feature, or simply mean that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
Claims (5)
1. A natural nicotine purification process is a production process which comprises the steps of preparing a tobacco extract raw material with 40% of nicotine content by using an anti-emulsifier, carrying out alkalization treatment, extraction separation, standing and settling, separating waste water, distilling and desolventizing, and rectifying and purifying until the nicotine content is more than or equal to 99.95% and the nicotine yield is more than or equal to 99.5%;
the devices or equipment required in each process comprise: the device comprises a batching tank, a mixing tank, an extraction tank, a settling tank, a pipeline filter, a clear liquid receiving tank, a pipeline sight glass, a No. 1 delivery pump, a distillation tower, a first condenser, a solvent recovery tank, a No. 2 delivery pump, a solvent cache tank, a feeding cache tank, a rectification tower pipe internally provided with stainless steel wire mesh filler, a second condenser, a condensate buffer tank, an automatic forced reflux distributor, a qualified product receiving tank, a unqualified product receiving tank, a reflux pipe, a sample collection valve and a rectification liquid collection pipe; the system also comprises a controller used for detecting and controlling the operation of each device or equipment: the system comprises a vacuum pump, a negative pressure pipeline, a cooling water circulating pipeline, a chilled water circulating pipeline, a heat conducting oil circulating pipeline, a temperature sensor, a pressure sensor, a flowmeter, a liquid level meter, an electric control valve and a centralized control system; the method is characterized in that:
the production process comprises the following steps:
stp1, preparation of an anti-emulsifier: injecting a set amount of purified water into the batching tank in a negative pressure mode, and then slowly adding caustic soda with a set amount and a purity of more than or equal to 98% while stirring to prepare an anti-emulsifier; controlling the adding time of the caustic soda to be more than or equal to 30min, stirring until the caustic soda is completely dissolved, and continuing stirring until the temperature of the anti-emulsifier in the batching tank is reduced to 40-45 ℃;
stp2, alkalization treatment: injecting raw materials to be purified into a mixing tank in a negative pressure suction mode, and slowly adding the anti-emulsifying agent prepared according to stp1 while stirring; controlling the adding time of the anti-emulsifying agent to be more than or equal to 30min, and continuously stirring for 90 to 120min after the anti-emulsifying agent is completely added into the tobacco extract; preparing an extract;
stp3, extraction and separation: injecting a set amount of normal hexane into an extraction tank in a negative pressure mode, and adding an extraction liquid prepared according to stp2 while stirring; controlling the adding time of the extract to be more than or equal to 60min, and continuously stirring for 90-150min after the extract is completely added; completing the extraction process to obtain an extraction mixed solution;
stp4, standing and settling: conveying the extraction mixed solution prepared according to stp3 to a settling tank in a negative pressure mode; the extraction mixed liquor is freely settled in a settling tank in a standing state, and the extraction mixed liquor is layered due to density difference and sequentially becomes clear liquid, emulsion and wastewater from top to bottom; the clear liquid is n-hexane solution extracted with nicotine;
setting: the free settling time of the extraction mixed solution in a standing state is more than or equal to 60 hours;
stp5, wastewater separation: observing the liquid level and the layering condition in the settling tank after stp4 reaches the set standing and settling time, and discharging the wastewater through a valve arranged at the bottom of the settling tank until the liquid level of the wastewater in the settling tank is lower than the height of a clear liquid discharge hole arranged on the settling tank; respectively discharging clear liquid, waste water and emulsion in a gravity self-flow mode, discharging the clear liquid into a clear liquid receiving tank, discharging the waste water into a temporary waste water treatment container, and discharging the emulsion for additional storage;
stp6, distillation desolventizing; conveying the clear liquid stored in the clear liquid receiving tank to a distillation tower in batches by a No. 1 delivery pump, separating n-hexane from the clear liquid in an evaporation and condensation mode, temporarily storing the separated n-hexane in a solvent recovery tank while distilling, and conveying the n-hexane to a solvent cache tank by a No. 2 delivery pump for extracting the raw materials of the next batch;
after the distillation desolventizing process is completed, what remains in the distillation column is: crude absolute oil with nicotine purity being more than or equal to 95 percent is conveyed to a feeding buffer tank in a negative pressure conveying mode;
setting: the distillation temperature of the clear liquid in the distillation tower is 80 to 140 ℃;
in the later stage of distillation, when the input flow of the solvent recovery tank is determined to be less than 1% of the maximum flow, closing an emptying valve arranged at the outlet of the solvent recovery tank, communicating the solvent recovery tank with an external vacuumizing pipeline, continuing distillation under the negative pressure condition, feeding nitrogen into the distillation tower for emptying until a thermometer arranged at the top of the distillation tower displays that the temperature does not fall or rise reversely, and closing a heating source;
stp7, rectification and purification: the rectification and purification comprises five links, which are respectively: feeding and balancing temperature, collecting front fraction, collecting high-purity nicotine, collecting rear fraction and recovering heavy clean oil;
in the rectification purification process, the flow ratio I between the return pipe and the rectification liquid pipe can be adjusted by adjusting a proportional adjustment three-way valve arranged in the automatic forced return distributor;
the specific operation process of the step is as follows:
a. feeding and equilibrium temperature: firstly, setting: the liquid flows through a condensate buffer tank and is totally refluxed to the upper end of a rectifying tower tube, namely the value I is infinite, and the vacuum degree in the rectifying tower is higher than-0.09 Mpa; pumping the crude clean oil fed into the buffer tank into a rectifying tower, heating to 135 +/-1 ℃, and setting the continuous evaporation and reflux time of the crude clean oil in the rectifying tower to be 3~4 hours under the constant temperature state;
b. collecting front fractions: regularly extracting a rectification liquid sample from the sample collection valve and analyzing, when the content of single high-boiling-point impurities in the rectification liquid is less than or equal to 100mg/kg, adjusting the I value = (5~3), and introducing the material flowing out of the rectification liquid pipe into a unqualified product receiving tank; when the purity of nicotine in the collected sample is more than or equal to 99.95 percent, the collection process of the front distillation is finished;
c. collecting high-purity nicotine fractions: keeping the value I as the set value in the step b, continuing rectification, when the purity of the nicotine in the collected sample is more than or equal to 99.95 percent, and the content of single high-boiling-point impurities is more than 100mg/kg but less than 200mg/kg, immediately guiding the material flowing out of the rectification liquid pipe 25 into the qualified product receiving tank 20, stopping collecting the high-purity nicotine fraction until the purity of the nicotine in the sample is reduced from high to 99.95 percent, and closing a feeding valve for communicating the qualified product receiving tank 20 with the rectification liquid pipe 25;
d. and (3) collecting the after fraction: after the step c is finished, adjusting the value I =0, namely cutting off reflux, and guiding the material flowing out of the rectification liquid pipe into a unqualified product receiving tank; d, continuously rectifying by the rectifying tower according to the temperature set in the step a until the temperature in the rectifying tower does not rise or fall reversely, and finishing the rectification; finally, returning the unqualified rectification liquid collected by the unqualified product receiving tank to the clear liquid receiving tank;
e. and (3) heavy clean oil recovery: after the rectification is finished, nitrogen is used for emptying and discharging heavy clean oil remained in the rectification tower, and then the next rectification circulation process is carried out.
2. The process of claim 1, wherein the step of purifying the natural nicotine comprises: the lower parts of the shells of the mixing tank and the material mixing tank are provided with cooling jackets which are used for accelerating the cooling of the materials stored in the mixing tank and the material mixing tank, and the cooling jackets are connected with a cooling water circulation pipeline arranged outside; the first condenser and the second condenser are also respectively connected with a cooling water circulation pipeline arranged outside; setting: the water inlet temperature of the circulating cooling water is less than or equal to 30 ℃, and the water return temperature is less than or equal to 35 ℃.
3. The process of claim 1, wherein the step of purifying the natural nicotine comprises: the lower parts of the shells of the qualified product receiving tank and the unqualified product receiving tank are provided with refrigeration jackets which are used for storing materials in the qualified product receiving tank and the unqualified product receiving tank under the low-temperature condition, and the refrigeration jackets are connected with a chilled water circulation pipeline arranged outside; setting: the water inlet temperature of the circulating chilled water is less than or equal to 5 ℃, and the water return temperature is less than or equal to 10 ℃.
4. The process of claim 1, wherein the step of purifying the natural nicotine comprises: in stp1, the following are set: the weight ratio of the purified water to the caustic soda is 4: (0.8 to 1.2); in stp2, the following are set: the weight ratio of the anti-emulsifier to the tobacco extract with the nicotine content accounting for 40% is 5: (3.5 to 4.5); in stp3, the following are set: the weight ratio of the n-hexane to the extract is 13: (8 to 10).
5. The process of claim 1, wherein the step of purifying the natural nicotine comprises: and in the stp5, the discharged emulsion is subjected to a shock demulsification method to further separate a clear liquid remaining in the emulsion, and the separated clear liquid is introduced into a clear liquid receiving tank.
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